Pyridine → HCID 58724547, 화합물

HRID 1393044노트

반응식

HRID 1393044 반응식
[CH3:1][N:2]1[C:6]([N:7]2[CH:11]=[CH:10][CH:9]=[CH:8]2)=[C:5]([C:12]([OH:14])=O)[CH:4]=[N:3]1.N1C=CC=CC=1.N1C(F)=NC(F)=NC=1[F:23]>ClCCl>[CH3:1][N:2]1[C:6]([N:7]2[CH:11]=[CH:10][CH:9]=[CH:8]2)=[C:5]([C:12]([F:23])=[O:14])[CH:4]=[N:3]1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 12664Cyanuric fluorideHCID 155002461-Methyl-5-(1H-pyrrol-1-yl)-1H-pyrazole-4-carboxylic acid

생성물 1

HCID 58724547HCID 58724547, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirred solution of 1-methyl-5-pyrrol-1-yl-1H-pyrazole-4-carboxylic acid (7.65 g, 40 mmol) in dry dichloromethane (150 mL) and pyridine (3.2 mL, 40 mmol) under a nitrogen atmosphere was added cyanuric fluoride (5.4 g, 40 mmol) at 0° C. The reaction mixture was stirred for two hours during which time the reaction temperature was allowed to rise to room temperature. Crushed ice was then added along with additional dichloromethane. The organic layer was separated and the aqueous layer was extracted twice with dichloromethane. Concentration of the combined organic layers under reduced pressure gave 1-methyl-5-pyrrol-1-yl-1H-pyrazole-4-carbonyl fluoride which was used in the next step without further purification.

후처리

  1. customto rise to room temperature
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted twice with dichloromethane

출처 및 근거

ORD 기록
ord-dde0e4045b7648f1953776d2217ab9d5
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07345058B2

반응 노트

불러오는 중…